Time-lapse scanning electron microscopy for measurement of contamination rate and stage drift

Measurements done with scanning electron microscopes (SEMs) may lose their validity due to contamination and charging caused by the primary electron beam. The sample stage and the electron beam also slightly drift during the course of the measurements. Consequently, it is essential to find out the time limit of valid measurements, that is, the maximum time before the sample or its position changes too much. This paper describes digital time-lapse SEM, a useful tool for investigating the extent and effects of contamination and stage drift. It works with hardware and software that create a stack of sequential images. Later these images can be viewed as a short movie; it is also possible to apply all the image processing and analysis procedures that are otherwise applied to separate, individual images. This method gives a reliable way of measuring the rate of contaminant deposition and of stage and electron beam drift of SEMs, and it could be helpful in controlling these problems.     

A high-resolution add-on in-lens attachment for scanning electron microscopes

A compact add-on objective lens for the scanning electron microscope (SEM) has been designed and tested. The lens is < 35 mm high and can be fitted on to the specimen stage as an easy-to-use attachment. Initial results show that it typically improves the spatial resolution of the SEM by a factor of three. The add-on unit is based upon a permanent magnet immersion lens design. Apart from the extra attachment to the specimen stage, the SEM with the add-on lens functions in the normal way. The in-lens unit can comfortably accommodate specimen heights up to 10 mm. The new add-on lens unit opens up the possibility of operating existing SEMs in the high-resolution in-lens mode. By using a deflector at the top of the add-on lens unit, it can also operate as a quantitative multichannel voltage contrast spectrometer, capable of recording the energy spectrum of the emitted secondary electrons. Initial experiments confirm that a significant amount of voltage contrast can be obtained.     

Mechanical scanning of the specimen in the scanning electron microscope

A scanning electron microscope (SEM) system equipped with a motor drive specimen stage fully controlled with a personal computer (PC) has been utilized for obtaining ultralow magnification SEM images. This modem motor drive stage works as a mechanical scanning device. To produce ultra-low magnification SEM images, we use a successful combination of the mechanical scanning, electronic scanning, and digital image processing techniques. This new method is extremely labor and time saving for ultra-low magnification and wide-area observation. The option of ultra-low magnification observation (while maintaining the original SEM functions and performance) is important during a scanning electron microscopy session.     

A simple cryo-holder facilitates specimen observation under a conventional scanning electron microscope

A pre-cryogenic holder (cryo-holder) facilitating cryo-specimen observation under a conventional scanning electron microscope (SEM) is described. This cryo-holder includes a specimen-holding unit (the stub) and a cryogenic energy-storing unit (a composite of three cylinders assembled with a screw). After cooling, the cryo-holder can continue supplying cryogenic energy to extend the observation time for the specimen in a conventional SEM. Moreover, the cryogenic energy-storing unit could retain appropriate liquid nitrogen that can evaporate to prevent frost deposition on the surface of the specimen. This device is proved feasible for various tissues and cells, and can be applied to the fields of both biology and material science. We have employed this novel cryo-holder for observation of yeast cells, trichome, and epidermal cells in the leaf of Arabidopsis thaliana, compound eyes of insects, red blood cells, filiform papillae on the surface of rat tongue, agar medium, water molecules, penicillium, etc. All results suggested that the newly designed cryo-holder is applicable for cryo-specimen observation under a conventional SEM without cooling system. Most importantly, the design of this cryo-holder is simple and easy to operate and could adapt a conventional SEM to a plain type cryo-SEM affordable for most laboratories.     

Imaging of specimens at optimized low and very low energies in scanning electron microscopes.

The modern trend towards low electron energies in scanning electron microscopy (SEM), characterised by lowering the acceleration voltages in low-voltage SEM (LVSEM) or by utilising a retarding-field optical element in low-energy SEM (LESEM), makes the energy range where new contrasts appear accessible. This range is further extended by a scanning low-energy electron microscope (SLEEM) fitted with a cathode lens that achieves nearly constant spatial resolution throughout the energy scale. This enables one to optimise freely the electron beam energy according to the given task. At low energies, there exist classes of image contrast that make particular specimen data visible most effectively or even exclusively within certain energy intervals or at certain energy values. Some contrasts are well understood and can presently be utilised for practical surface examinations, but others have not yet been reliably explained and therefore supplementary experiments are needed.     

Pressure effect of growing with electron beam-induced deposition with tungsten hexafluoride and tetraethylorthosilicate precursor

Electron beam-induced deposition (EBID) provides a simple way to fabricate submicron- or nanometer-scale structures from various elements in a scanning electron microscope (SEM). The growth rate and shape of the deposits are influenced by many factors. We have studied the growth rate and morphology of EBID-deposited nanostructures as a function of the tungsten hexafluoride (WF6) and tetraethylorthosilicate (TEOS) precursor gas pressure and growth time, and we have used Monte Carlo simulations to model the growth of tungsten and silicon oxide to elucidate the mechanisms involved in the EBID growth. The lateral radius of the deposit decreases with increasing pressure because of the enhanced vertical growth rate which limits competing lateral broadening produced by secondary and forward-scattered electrons. The morphology difference between the conical SiO(x) and the cylindrical W nanopillars is related to the difference in interaction volume between the two materials. A key parameter is the residence time of the precursor gas molecules. This is an exponential function of the surface temperature; it changes during nanopillar growth and is a function of the nanopillar material and the beam conditions.     

A portable scanning electron microscope column design based on the use of permanent magnets

A portable scanning electron microscope (SEM) column design is presented which makes use of permanent magnets. Simulation results predict that such an SEM column is feasible and that it can be compact. The column height is typically less than 12 cm. The column is designed to be modular, so that it can fit onto a wide range of different specimen chamber types, and can also be readily replaced.     

A high signal-to-noise ratio toroidal electron spectrometer for the SEM

This paper presents a high signal-to-noise ratio electron energy spectrometer attachment for the scanning electron microscope (SEM), designed to measure changes in specimen surface potential from secondary electrons and extract specimen atomic number information from backscattered electrons. Experimental results are presented, which demonstrate that the spectrometer can in principle detect specimen voltage changes well into the sub-mV range, and distinguish close atomic numbers by a signal-to-noise ratio of better than 20. The spectrometer has applications for quantitatively mapping specimen surface voltage and atomic number variations on the nano-scale.     

Optimisation of the environmental scanning electron microscope for observation of drying of matt water-based lacquers

Environmental scanning electron microscopy (ESEM) modifies conventional SEM through the use of a partial gas pressure in the microscope specimen chamber. Like conventional SEM, it has the resolution to image structure on the submicron lengthscale, but can also tolerate hydrated specimens if water vapour is used in the specimen chamber. This ability to image aqueous specimens leaves ESEM uniquely placed to study in situ drying in polymer latexes. However, there are two key practical difficulties associated with in situ drying. First, the size of the latex particles: larger latex particles are typically around 500 nm in diameter. Although ESEM can resolve structure on this lengthscale without difficulty, the magnification required results in radiation damage of the specimen due to the electron beam. This means that a given region can be imaged only once during film formation, so the evolution of particular features cannot be followed. Second, the change from ambient temperature and pressure to the ESEM conditions of 7 degrees C and 7.5 torr (100 Pa) can subject the specimen to a very high evaporation rate, which can disrupt film formation. The inclusion of a drop of water in the specimen chamber is shown largely to alleviate this, enabling successful imaging of film formation in the lacquer. Instead of the polymer latex itself, this work concentrates on a matting lacquer with silica inclusions. The silica matting agent particles are 1-10 microm in size, allowing for a lower magnification to be used, massively reducing specimen damage. Furthermore, the contrast during drying is much enhanced in the presence of silica. The images reveal the silica as bright regions against a darker background of polymer and water. Film formation shows the transition from a uniform, featureless aqueous solution to a polymer film with silica particles present on the surface. The appearance of individual silica particles can be followed. The particles are generally revealed quite early, after a few minutes of drying time. As film formation progresses, these same particles appear larger and more distinct. Few new particles are revealed at longer film formation times.     

A study of electron beam-induced conductivity in resists.

The charging of polymeric resist materials during electron beam irradiation leads to significant problems during imaging and lithography processes. Charging occurs because of charge deposition in the polymer and charge generation/trapping due to formation of electron-hole pairs in the dielectric. The presence of such charge also results in the phenomena of electron beam-induced conductivity (EBIC). Electron beam-induced conductivity data have been obtained for three commercial e-beam resists under a variety of dose rate and temperature conditions. From the observed values of induced conductivity under varying conditions significant information about the generation of electron-hole pair and the transport of charge in the resist can be obtained. Three electron beam resists, EBR900, ZEP7000, and PBS are examined by an external bias method. The difference in resist chemistry is considered to play the role in the initial state EBIC behaviors among three resists even though the way that it affects the behaviors is not clear. A comparison of the power consumption comparison is proposed as a measure to give a preliminary estimate of the carrier concentration and carrier drift velocity differences among the resists. A simple single trap model with constant activation energy is proposed and provides good agreement with experiment.     

Scanning electron microscope charging effect model for chromium/quartz photolithography masks

We propose a new method for fitting a model of specimen charging to scanning electron microscope (SEM) images. Charging effects cause errors when one attempts to infer the size or shape of a specimen from an image. The goal of our method is to enable image analysis algorithms for measurement, segmentation, and three-dimensional (3-D) reconstruction that would otherwise fail on images containing charging effects. Our model is applied to images of chromium/quartz photolithography masks and may also work in the more general case of isolated metal islands on a flat insulating substrate. Unlike methods based on Monte Carlo simulation, our simulation method does not handle more general topographies or specimens composed entirely of an insulator; it is a crude approximation to the physical charging process described in more detail in Cazaux (1986) and Melchinger and Hofmann (1985), but can be fit with quantitative accuracy to real SEM images. We only consider changes in intensity and do not model charging-induced distortion of image coordinates. Our approach has the advantage over existing methods of enabling fast prediction of charging effects so it may be more practical for image analysis applications.     

Contamination in a scanning electron microscope and the influence of specimen cooling

Solutions of the stationary and time-dependent equations of diffusion are presented for contamination when scanning a rectangular area in the scanning electron microscope (SEM). A method is described to record the thickness of the contamination layer by the signal of secondary or backscattered electrons and to measure the influence of electron current density, beam energy, and specimen cooling on the contamination rate.     

The remote electron beam-induced current analysis of grain boundaries in semiconducting and semi-insulating materials

When no charge collecting p-n junction or Schottky barrier is present in the specimen, but two contacts are applied, conductive mode scanning electron microscope (SEM) observations known as remote electron beam-induced current (REBIC) can be made. It was described as "remote" EBIC because the contacts to the specimen can lie at macroscopic distances from the beam impact point. In recent years, REBIC has been found to be useful not only for studies of grain boundaries in semiconducting silicon and germanium, but also in semi-insulating materials such as the wider bandgap II-VI compounds and electroceramic materials like varistor ZnO and positive temperature coefficient resistor (PTCR) BaTiO3. The principles of this method are outlined. Accounts are given of the five forms of charge collection and resistive contrast that appear at grain boundaries (GBs) in REBIC micrographs. These are (1) terraced contrast due to high resistivity boundary layers, (2) peak and trough (PAT) contrast due to charge on the boundary, (3) reversible contrast seen only under external voltage bias due to the beta-conductive effect in a low conductivity boundary layer, (4) dark contrast due to enhanced recombination, and (5) bright contrast apparently due to reduced recombination. For comparison, the results of the extensive EBIC studies of GBs in Si and Ge are first outlined and then the results of recent REBIC grain boundary studies in both semiconducting and semi-insulating materials are reviewed.     

A portable cryo-storage system for low-temperature scanning electron microscopy,suitable for international transport of cryo-specimens

A cryo-specimen storage system for low-temperature scanning electron microscopy (LTSEM) specimens is described, which: liberates multi-specimen experiments from sampling restrictions imposed by the rate at which LTSEM specimens can be examined in the SEM; provides security against experiment loss resulting from breakdown of the SEM or cryo-system; enables collection of specimens in the field or in laboratories remote from the SEM laboratory; and facilitates international air transport of LTSEM specimens. The components of the system, which has a capacity of 98 stub-mounted specimens, are readily made in a laboratory workshop. The details of the design may be altered to suit particular specimen types or experimental approaches.     

Use of backscattered electron detector arrays for forming backscattered electron images in the scanning electron microscope

The backscattered electron (BSE) signal in the scanning electron microscope (SEM) can be used in two different ways. The first is to give a BSE image from an area that is defined by the scanning of the electron beam (EB) over the surface of the specimen. The second is to use an array of small BSE detectors to give an electron backscattering pattern (EBSP) with crystallographic information from a single point. It is also possible to utilize the EBSP detector and computer-control system to give an image from an area on the specimen--for example, to show the orientations of the grains in a polycrystalline sample ("grain orientation imaging"). Some further possibilities based on some other ways for analyzing the output from an EBSP detector array, are described.     

Scanning electron microscopic technique for imaging a diamond tool edge

A technique is described to measure the edge radius of diamond cutting tools using the scanning electron microscope (SEM). This method attempts to overcome two major limitations of the SEM in this application: low image contrast and lack of quantitative topographic information. A line of electron beam contamination, viewed at an angle, provides improved contrast for focusing and a means of obtaining the tool profile from the geometry.     

Use of Monte Carlo modeling for interpreting scanning electron microscope linewidth measurements

A scanning electron microscope (SEM) can be used to measure the dimensions of the microlithographic features of integrated circuits. However, without a good model of the electron-beam/specimen interaction, accurate edge location cannot be obtained. A Monte Carlo code has been developed to model the interaction of an electron beam with one or two lines lithographically produced on a multilayer substrate. The purpose of the code is to enable one to extract the edge position of a line from SEM measurements. It is based on prior codes developed at the National Institute of Standards and Technology, but with a new formulation for the atomic scattering cross sections and the inclusion of a method to simulate edge roughness or rounding. The code is currently able to model the transmitted and backscattered electrons, and the results from the code have been applied to the analysis of electron transmission through gold lines on a thin silicon substrate, such as is used in an x-ray lithographic mask. Significant reductions in backscattering occur because of the proximity of a neighboring line.     

Topographic and material contrast in low-voltage scanning electron microscopy

Two scintillation backscattered electron (BSE) detectors with a high voltage applied to scintillators were built and tested in a field emission scanning electron microscope (SEM) at low primary beam energies. One detector collects BSE emitted at low take-off angles, the second at high takeoff angles. The low take-off detector gives good topographic tilt contrast, stronger than in the case of the secondary electron (SE) detection and less sensitive to the presence of contamination layers on the surface. The high take-off detector is less sensitive to the topography and can be used for detection of material contrast, but the contrast becomes equivocal at the beam energy of 1 keV or lower.